反应详情

Sodium hydride (60% dispersion in mineral oil, 8.2 g, 205 mmol) was added to a mixture of 6-amino-2-methoxy-4-pyrimidone (24.0 g, 170 mmol) in DMF at 0° C. After 0.5 hours, lithium bromide (19.2 g, 221 mmol) was added to the mixture and stirred for 0.5 hours at room temperature. The temperature was slowly increased to 70° C., and a solution of 4-bromobutyl acetate (50 g, 256 mmol) in DMF was added dropwise to the reaction mixture. The mixture was stirred at 70° C. for 3 hours. After cooling to room temperature, the solvent was removed in vacuo. The residue was purified by chromatography on silica gel using CHCl3/MeOH (1-5%) as eluent to give first 6.5 g (15%) of 6-amino-2-methoxy-4-(4-acetoxybutyl)pyrimidine as a white solid followed by 23.4 g (yield 54%) of 6-amino-2-methoxy-3-(4-acetoxybutyl)-4-pyrimidone as a white solid.

1. temperatureThe temperature was slowly increased to 70° C.
2. stirringThe mixture was stirred at 70° C. for 3 hours
3. temperatureAfter cooling to room temperature
4. customthe solvent was removed in vacuo
5. customThe residue was purified by chromatography on silica gel